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Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite

A lithium iron phosphate and precursor technology is applied in the field of comprehensively utilizing ilmenite to prepare lithium iron phosphate precursors for cathode materials of lithium ion batteries, and achieves the effects of simple process flow, stable product quality and good product quality.

Inactive Publication Date: 2008-09-17
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no reports on the comprehensive utilization of ilmenite to prepare lithium iron phosphate precursors for lithium-ion battery cathode materials

Method used

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  • Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite
  • Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Leach 1kg of ilmenite with sulfuric acid, filter to obtain filtrate, dissolve a certain amount of hematite and ferric sulfate in the filtrate, so that the concentration of Fe in the mixed solution is 0.1mol / L, and the molar ratio of Ti to Fe is 0.5; Add an appropriate amount of 0.01mol / L sodium peroxide solution to the mixed solution, adjust the pH of the system to about 1.5 with 0.5mol / L sodium hydroxide solution, stir for a few minutes and filter to obtain the filtrate; add an appropriate amount of 1mol / L ammonium carbonate solution, adjust the pH of the system to about 6.0 with 2mol / L ammonia water, react in a stirred reactor at 50°C for 10min, filter, wash, dry the precipitate at 100°C and put it in the air Calcining at 600° C. for 2 hours to obtain the precursor of lithium iron phosphate, the anode material of the lithium ion battery, and the ferric oxide of the doped metal element.

Embodiment 2

[0029] Leach 1 kg of ilmenite with hydrochloric acid, filter to obtain the filtrate, dissolve a certain amount of ferric chloride in the filtrate, so that the concentration of Fe in the mixed solution is 1mol / L, and the molar ratio of Ti to Fe is 0.3; Add an appropriate amount of 3mol / L sodium hypochlorite solution, adjust the pH of the system to about 3.0 with a 2mol / L lithium hydroxide solution, and filter after stirring for several minutes to obtain a filtrate; add an appropriate amount of 2mol / L sodium carbonate solution in the filtrate, and use 0.1mol / L sodium hydroxide solution to adjust the pH of the system to about 4.0, react in a stirred reactor at 10°C for 4h, filter and wash, dry the precipitate at 50°C, and then calcinate at 800°C in air for 1h That is, the precursor of the positive electrode material lithium iron phosphate of the lithium ion battery-the ferric oxide of the doped metal element is obtained.

Embodiment 3

[0031] Leach 1 kg of ilmenite with sulfuric acid, filter to obtain the filtrate, dissolve a certain amount of ferrous sulfate and ferrous chloride in the filtrate, so that the concentration of Fe in the mixed solution is 2mol / L, and the molar ratio of Ti to Fe is 0.1 Add an appropriate amount of 1mol / L potassium chlorate solution to the mixed solution, adjust the pH of the system to about 6.0 with 3mol / L ammonia water, filter after stirring for several minutes, and obtain the filtrate; add an appropriate amount of 3mol / L potassium bicarbonate to the filtrate Solution, use 6mol / L potassium hydroxide solution to adjust the pH of the system to about 14.0, react in a stirred reactor at 70°C for 2h, filter and wash, dry the precipitate at 150°C, and then calcinate in air at 300°C After 24 hours, the precursor of lithium iron phosphate, the cathode material of the lithium ion battery, is obtained—the ferric oxide of the doped metal element.

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Abstract

The invention discloses a preparation method for lithium iron phosphate precursor by comprehensively utilizing ilmenite, comprising a plurality of steps: leach the ilmenite in acid and filtrate is obtained by filtering; dissolve a certain amount of other iron sources in the filtrate to make the Fe concentration in the mixed solution as 0.01-3mol / L and the molar ratio of Ti and Fe as 0.0005-0.5; add appropriate amount of oxidant to the mixed solution; use alkali aqueous solution to regulate the system pH as 4.0-14.0; react for 10min to 24h at 10-90 DEG Cin a stir reactor; filter, wash and dry the sedimentation at 50-159 DEG C; after drying, calcine the sedimentation in air at 300-800 DEG C for 1-24h; lithium iron phosphate precursor for the lithium-ion battery cathode material, which is also the ferric oxide of doped-metal elements, can be obtained. The preparation method has the advantages of wide material source, simple technological process, good and stable product quality and low cost.

Description

technical field [0001] The invention relates to a preparation method of a lithium iron phosphate precursor for a positive electrode material of a lithium ion battery, in particular to a method for comprehensively utilizing ilmenite to prepare a lithium iron phosphate precursor for a positive electrode material of a lithium ion battery. technical background [0002] Lithium iron phosphate with an olivine structure has become one of the most promising cathode materials for lithium-ion batteries due to its high theoretical specific capacity (170mAh / g), good cycle performance, good thermal stability, low price, and environmental friendliness. . However, as the main raw material for the production of lithium iron phosphate-iron salt, the large-scale industrial production of lithium iron phosphate is seriously restricted due to shortcomings such as unstable product quality, low density, and low purity. [0003] At present, most of the iron sources for preparing lithium iron phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/10
Inventor 王志兴伍凌李新海郭华军彭文杰胡启阳张云河刘久清李灵均符芳铭
Owner CENT SOUTH UNIV
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